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Potassium Carbonate → 5-(4,4-diethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-1-methyl-1H-pyrrole-2-carbonitrile

HRID 458558
ノート
印刷プレビュー

反応式

HRID 458558 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7]#[N:8].C(OB(OC(C)C)OC(C)C)(C)C.C([N-]C(C)C)(C)C.[Li+].Br[C:31]1[CH:45]=[CH:44][C:34]2[NH:35][C:36](=[O:43])[O:37][C:38]([CH2:41][CH3:42])([CH2:39][CH3:40])[C:33]=2[CH:32]=1.C(=O)([O-])[O-].[K+].[K+].[Cl-].[NH4+]>C1COCC1.O>[CH2:41]([C:38]1([CH2:39][CH3:40])[C:33]2[CH:32]=[C:31]([C:6]3[N:2]([CH3:1])[C:3]([C:7]#[N:8])=[CH:4][CH:5]=3)[CH:45]=[CH:44][C:34]=2[NH:35][C:36](=[O:43])[O:37]1)[CH3:42]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 11430Potassium CarbonateHCID 21531Triisopropyl borateHCID 25517Ammonium ChlorideHCID 20641111-Methylpyrrole-2-carbonitrileHCID 2724682Lithium diisopropylamideHCID 112775676-Bromo-4,4-diethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one

生成物 1

HCID 11255323
5-(4,4-diethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-1-methyl-1H-pyrrole-2-carbonitrile
収率 55.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 1-methyl-1H-pyrrole-2-carbonitrile (4.1 g, 35 mmol) and triisopropylborate (8.9 mL, 38.5 mmol) in THF (80 mL) at 0° C. was added lithium diisopropylamide (22.8 mL, 45.5 mmol). The reaction mixture was allowed to warm to room temperature. Upon completion by TLC, the reaction was added dropwise to a 65° C. solution of 6-bromo-4,4-diethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one (2.0 g, 7.0 mmol), potassium carbonate (2.9 g, 21 mmol) dissolved in (25 mL water), and tetrakistriphenylphosphine palladium (0) (0.4 g, 0.35 mmol) in tetrahydrofuran (20 mL). Upon completion by TLC of the reaction, it was poured into a saturated solution of ammonium chloride (200 mL), extracted with ethyl acetate (100 mL), dried with magnesium sulfate, and concentrated. Trituration of the residue with ethyl acetate/dichloromethane gave 5-(4,4-diethyl-2-oxo-1,4-dihydro-2H-3,1-benzoxazin-6-yl)-1-methyl-1H-pyrrole-2-carbonitrile (1.2 g, 55%) as an off-white solid. 1H NMR (DMSO-d6): δ10.26 (s, 1H), 7.37 (d, 1H, J=8.2, 1.6 Hz), 7.31 (d, 1H, J=1.8 Hz), 7.03 (d, 1H, J=4.0 Hz), 6.96 (d, 1H, J=8.2 Hz), 6.32 (d, 1H, J=4.0 Hz), 3.69 (s, 3H), 2.02 (m, 2H, J=7.3 Hz), 1.88 (m, 2H, J=7.3 Hz), 0.78 (t, 6H, J=7.3 Hz). MS (ESI) m/z 310 ([M+H]+); MS (ESI) m/z 308 ([M−H]−). HRMS: calcd for C18H19N3O2, 309.1477; found (ESI_FT), 310.15488;

後処理

  1. customUpon completion by TLC of the reaction, it
  2. extractionextracted with ethyl acetate (100 mL)
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-a6d2224085c34cb88297cdb878dd21b0
出典データセット
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07192956B2

反応ノート

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